CN107994222A - A kind of sandwich structure C-base composte material and its preparation method and application - Google Patents
A kind of sandwich structure C-base composte material and its preparation method and application Download PDFInfo
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- CN107994222A CN107994222A CN201711276189.7A CN201711276189A CN107994222A CN 107994222 A CN107994222 A CN 107994222A CN 201711276189 A CN201711276189 A CN 201711276189A CN 107994222 A CN107994222 A CN 107994222A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation method of sandwich structure C-base composte material, comprise the following steps：(1) chitosan is uniformly mixed with zincum salts pore creating material, through carbonization treatment, obtains porous carbon nanosheet；(2) porous carbon nanosheet obtained by step (1) is immersed in soluble nickel salting liquid, takes out drying, be vapor-deposited through CVD, up to sandwich structure C-base composte material.The preparation method raw material is easy to get, is reproducible, being easily industrialized production.The invention discloses a kind of sandwich structure C-base composte material, the C-base composte material good conductivity.The invention also discloses application of the above-mentioned sandwich structure C-base composte material as negative material in sodium-ion battery, the sodium-ion battery specific capacity height made of the C-base composte material of this law, good rate capability, good cycle.
Description
Technical field
The present invention relates to sodium-ion battery technical field, and in particular to a kind of sandwich structure C-base composte material and its system
Preparation Method and application.
Background technology
Sodium-ion battery relies on sodium rich reserves, can use for reference the advantages such as existing battery achievement, become secondary cell of new generation
The research hotspot of system.Although the reaction mechanism in sodium-ion battery is similar to lithium ion battery, however, sodium ion radius ratio
Lithium ion wants big by 55% or so, insertion of the sodium ion in identical structural material and diffusion often all relative difficulty, electrode material
Decide the important parameter such as capacity, operating voltage and the cycle life of battery, thus the specific capacity of electrode material, kinetics
Energy and cycle performance etc. are all correspondingly deteriorated.Therefore preferably sodium-ion battery needs larger interlayer with embedded type negative material
Away from.
In existing anode material of lithium-ion battery, carbon material is that research is also the more negative material of research earliest.Without fixed
Type carbon material is high by its specific capacity, the advantages that having extended cycle life, becomes and studies more carbon material species.For agraphitic carbon
Storage sodium capacity is mainly derived from avtive spot, low graphitization crystallite area and micropore area etc., however amorphous carbon material as sodium from
Sub- cell negative electrode material, the problem of in the prevalence of poorly conductive and poor high rate performance, seriously inhibits agraphitic carbon as sodium
The application of ion battery anode.The structure of material has an immense impact on material electrochemical performance, therefore, to amorphous carbon material
It is to solve an existing Carbon negative electrode material of sodium ion battery important directions of problems to carry out structure and graphitization regulation and control.
The content of the invention
For the deficiency and defect mentioned in background above technology, be easy to get it is an object of the present invention to provide a kind of raw material,
The preparation method of sandwich structure C-base composte material that is reproducible, being easily industrialized production.
It is a further object of the invention to provide the high sandwich structure carbon of a kind of electron conduction and ionic mobility
Based composites.
It is a further object of the invention to provide a kind of above-mentioned sandwich structure C-base composte material in sodium-ion battery
In application.Negative material using the C-base composte material as sodium-ion battery, gained sodium-ion battery specific capacity is high, multiplying power
Performance is good, good cycle.
In order to solve the above technical problems, technical solution proposed by the present invention is：
In the present invention, the preparation method of sandwich structure C-base composte material, comprises the following steps：
(1) chitosan is uniformly mixed with zincum salts pore creating material, through carbonization treatment, obtains porous carbon nanosheet；
(2) porous carbon nanosheet obtained by step (1) is immersed in soluble nickel salting liquid, drying is taken out, through CVD gas phases
Deposition, up to sandwich structure C-base composte material.
The present invention uses zincum salts pore creating material, using chitosan as carbon source, porous carbon nanosheet is prepared through carbonization treatment
Material.Zincum salts pore creating material is used as from sacrifice template and decomposes and gasify in carbonisation, is formed in carbon material a large amount of small
Hole, obtains the carbon nanosheet material with loose structure.Porous carbon nanosheet is immersed in soluble nickel salting liquid again, is taken
Go out drying, nickel ion is uniformly attached on porous carbon nanosheet by liquid phase method, realize the uniformly negative of catalyst (nickel ion)
Carry；In CVD vapor deposition processes, by the catalytic action of nickel, graphitized carbon homoepitaxial is in porous carbon nanosheet surface, shape
Into the sandwich structure of graphitization carbon-coating cladding amorphous carbon layer, the formation of graphitization carbon-coating has beneficial to the electrical property for improving material
Energy；In addition, the thickness of accurately control graphitization carbon-coating is also allowed for using CVD vapour deposition processes, so as to fulfill to carbon-based composite wood
Expect careful design and the regulation and control of structure.
Sandwich structure C-base composte material porosity as obtained by the method for the present invention is high, and interlamellar spacing is moderate, reaction
Avtive spot enriches, good with electrolyte wetability, provides good dynamic conditions for sodium ion and electrolyte transmission, has good
Good sodium ion is embedded and abjection ability, good conductivity, the sandwich structure C-base composte material have concurrently highly electron conductive and
Ionic mobility is, it can be achieved that the Rapid reversible storage of sodium ion.
Preferably, in step (2), the condition of CVD vapour depositions is：C2H2Airflow rate is 1~100mL/min, argon gas
Airflow rate is 10~1000mL/min, and vapour deposition temperature is 700~1000 DEG C, and vapor deposition times are 0.5~5h.Herein
Under the conditions of gained sandwich structure C-base composte material in graphitization carbon-coating thickness it is moderate.
Further preferably, vapor deposition times are 1~5h.
Preferably, in step (2), soluble nickel salt is the one or more in nickel chloride, nickel nitrate and nickel acetate.
More preferably nickel chloride.
Preferably, in step (2), the concentration of soluble nickel salting liquid is 0.01~1mol/L.
More preferably 0.05~1mol/L.
Still more preferably it is 0.5~1mol/L.
Preferably, in step (1), the temperature of carbonization treatment is 500~1200 DEG C.
Preferably, in step (1), the time of carbonization treatment is 0.5~5h.
More preferably 1~5h.
Still more preferably it is 2~5h.
Preferably, in step (1), the mixing is specifically referred to chitosan and zincum salts pore creating material ball in the ball mill
Grind 1~20h.
More preferably 4~20h of ball milling.
Preferably, in step (1), the mass ratio of chitosan and zincum salts pore creating material is 1：(1~100).
More preferably 1：(10~100).
Preferably, in step (1), zincum salts pore creating material is the one or more in zinc acetate, zinc chloride and zinc nitrate.
More preferably zinc nitrate.
Preferably, in step (2), the time of immersion is 1~20h.
More preferably 2~20h.
Still more preferably it is 5~20h.
Present invention also offers a kind of sandwich structure C-base composte material, the C-base composte material is by above-mentioned preparation side
Method is prepared.The C-base composte material forms sandwich structure by graphitization carbon-coating cladding amorphous carbon layer, its outer layer is stone
Inkization carbon material, internal layer are amorphous carbon material.
As preferable scheme, the thickness of the graphitization carbon-coating is 1~100nm, and the thickness of the amorphous carbon layer is
10~200nm.
Further preferred scheme, the thickness of graphitization carbon-coating are 20~100nm, the thickness of amorphous carbon layer for 10~
100nm。
Another aspect of the present invention additionally provides a kind of application of above-mentioned sandwich structure C-base composte material, as negative
Pole materials application is in sodium-ion battery.Sandwich structure C-base composte material prepared by the present invention is used as working electrode, with
Sodium is to electrode, is assembled into button cell.
Under the current density of 50mA/g, the cycle performance of button cell is tested；Surveyed under the current density of 2000mA/g
Try the high rate performance of button cell.Test result shows, the electricity of sandwich structure C-base composte material assembling using the present invention
Pond has good chemical property：Under the current density of 50mA/g, after the circle of circulation 50, remain to keep the ratio of more than 300mA/g
Capacity；Under the power-discharging density of 2000mA/g, remain to keep the specific capacity of more than 100mAh/g.
Compared with prior art, the advantage of the invention is that：
(1) preparation method of the invention using the chitosan and zincum salts pore creating material being easy to get respectively as carbon source and template,
Porous carbon nanometer sheet material is obtained through carbonization treatment, zinc salt is decomposed and gasified by carbonization as pore creating material and from template is sacrificed,
Make carbon material that there is loose structure, while exempt template process, environmentally protective, raw material is easy to get, cost is low.
(2) preparation method of the invention adheres to nickel salt catalyst using liquid phase method on porous carbon nanosheet, then passes through CVD
Vapour deposition forms graphitization carbon-coating on porous carbon nanosheet surface, and accurately controls graphitized carbon layer thickness, forms graphite
Change the sandwich structure of carbon-coating cladding agraphitic carbon, this method technique is simple, and favorable reproducibility is environmental-friendly, is adapted to industry metaplasia
Production.
(3) preparation method of the invention using two-step method obtain reactivity site enrich, interlamellar spacing it is moderate, porosity
Height, the sandwich structure C-base composte material of good conductivity, the C-base composte material have as the negative material of sodium-ion battery
There is excellent electric property.
(4) sandwich structure carbon-based material of the invention overcomes the reactivity site of existing carbon material generally existing and lacks
The problem of weary and interlamellar spacing is excessive or too small, the good conductivity of sandwich structure carbon-based material, interlamellar spacing is moderate, reaction active site
Point is abundant, and sodium ion transmission dynamics is excellent, and problem of being shunk to volumetric expansion caused by sodium ion insertion deintercalation provides good
Alleviate, gained sandwich structure carbon-based material storage sodium excellent performance.
(5) sandwich structure C-base composte material of the invention is used in sodium-ion battery as negative material, gained sodium
Ion battery has the advantages that specific capacity height, good rate capability, good cycle.
To sum up, the preparation method technique of the present invention is simple, favorable reproducibility, raw material are easy to get, cost is low, it is environmentally protective,
It is suitable for industrialized production；The C-base composte material of the present invention has sandwich structure, and reactivity site is enriched, interlamellar spacing is fitted
In, porosity is high, good conductivity；The sodium-ion battery specific capacity that sandwich structure C-base composte material using the present invention makes
Height, good rate capability, good cycle, it is under the current density of 50mA/g, after the circle of circulation 50, remains to keep more than 300mA/g
Specific capacity；Under the power-discharging density of 2000mA/g, remain to keep the specific capacity of more than 100mAh/g.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of sandwich structure C-base composte material made from the embodiment of the present invention 1.
Embodiment
For the ease of understanding the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood implication of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
Chitosan 1g and zinc nitrate 10g are placed in ball grinder, ball milling 5h, by 600 DEG C of carbonizations, by washing and ethanol
Washing obtains porous carbon nanometer sheet material.
Porous carbon nanometer sheet material obtained by 0.2g is placed in the nickel chloride solution that concentration is 0.1mol/L and soaks 1h, is passed through
After freeze-drying, gained presoma is placed in CVD (chemical vapor deposition) system, controls C2H2Airflow rate is 1mL/min,
Argon stream speed is 100mL/min, and temperature is 700 DEG C, time 5h.Resulting materials obtain Sanming City afterwards by washing is dry
Control structure C-base composte material.Its graphitized carbon layer thickness is about 10nm, and agraphitic carbon layer thickness is about 200nm.Gained Sanming City
The scanning electron microscope (SEM) photograph for controlling structure C-base composte material is as shown in Figure 1.
Sandwich structure C-base composte material manufactured in the present embodiment is used as working electrode, sodium is to electrode, is assembled into
Button cell.Under the current density of 50mA/g, the cycle performance of battery is tested；Electricity is tested under the current density of 2000mA/g
The high rate performance in pond.Test result shows that the sodium-ion battery has good chemical property：In the current density of 50mA/g
Under, after the circle of circulation 50, remain to keep the specific capacity of 301mAh/g；Under the power-discharging density of 2000mA/g, remain to keep 110mAh/
The specific capacity of g.
Embodiment 2：
Chitosan 1g and zinc nitrate 100g are placed in ball grinder, ball milling 5h, by 1200 DEG C of carbonizations, by washing and second
Alcohol washs to obtain porous carbon nanometer sheet material.
Porous carbon nanometer sheet material obtained by 0.2g is placed in the nickel chloride solution that concentration is 1mol/L and soaks 10h, is passed through
After freeze-drying, gained presoma is placed in CVD system, controls C2H2Airflow rate is 100mL/min, argon stream speed
For 1000mL/min, temperature is 1000 DEG C, time 1h.It is carbon-based that resulting materials obtain sandwich structure after washing drying
Composite material.Its graphitized carbon layer thickness is about 80nm, and agraphitic carbon layer thickness is about 100nm.
Sandwich structure carbon-based material manufactured in the present embodiment is used as working electrode, sodium is to electrode, is assembled into button
Battery, under the current density of 50mA/g, test loop performance；The forthright again of battery is tested under the current density of 2000mA/g
Energy.Test result shows that sodium-ion battery prepared by this example has good chemical property：In the current density of 50mA/g
Under, after the circle of circulation 50, remain to keep the specific capacity of 321mAh/g；Under the power-discharging density of 2000mA/g, remain to keep respectively
The specific capacity of 147mAh/g.
Embodiment 3：
Chitosan 1g and zinc nitrate 20g are placed in ball grinder, ball milling 4h, by 1000 DEG C of carbonizations, by washing and second
Alcohol washs to obtain porous carbon nanometer sheet material.Gained 0.2g porous carbon nanometer sheet materials are placed on the chlorination that concentration is 0.5mol/L
5h is soaked in nickel solution, after freeze-drying, gained presoma is placed in CVD system, controls C2H2Airflow rate is
10mL/min, argon stream speed are 100mL/min, and temperature is 800 DEG C, time 3h.Resulting materials are by washing drying
After obtain sandwich structure carbon-based material.Graphitized carbon layer thickness is 50nm, and agraphitic carbon layer thickness is 150nm.
Sandwich structure C-base composte material manufactured in the present embodiment is used as working electrode, sodium is to electrode, is assembled into
Button cell.Under the current density of 50mA/g, the cycle performance of battery is tested；Electricity is tested under the current density of 2000mA/g
The high rate performance in pond.Test result shows that the sodium-ion battery has good chemical property：In the current density of 50mA/g
Under, after the circle of circulation 50, remain to keep the specific capacity of 335mAh/g；Under the power-discharging density of 2000mA/g, remain to keep 140mAh/
The specific capacity of g.
Comparative example 1：
This comparative example and embodiment difference lies in, porous carbon nanosheet is not immersed in nickel chloride solution, and without
CVD is vapor-deposited.
Chitosan 1g and zinc nitrate 10g are placed in ball grinder, ball milling 5h, by 600 DEG C of carbonizations, then by washing and second
Alcohol washs to obtain porous carbon nanometer sheet material.
Porous carbon nanometer sheet material prepared by this comparative example is used as working electrode, sodium is to electrode, is assembled into button electricity
Pond, under the current density of 50mA/g, tests the cycle performance of battery；Times of battery is tested under the current density of 2000mA/g
Rate performance.Test result shows：Under the current density of 50mA/g, after the circle of circulation 50, it is only capable of keeping the specific capacity of 203mAh/g；
Under the power-discharging density of 2000mA/g, it is only capable of keeping the specific capacity of 76mAh/g.
Claims (10)
1. a kind of preparation method of sandwich structure C-base composte material, comprises the following steps：
(1) chitosan is uniformly mixed with zincum salts pore creating material, through carbonization treatment, obtains porous carbon nanosheet；
(2) porous carbon nanosheet obtained by step (1) is immersed in soluble nickel salting liquid, takes out drying, sink through CVD gas phases
Product, up to sandwich structure C-base composte material.
2. the preparation method of sandwich structure C-base composte material according to claim 1, it is characterised in that the step
(2) in, the condition of CVD vapour depositions is：C2H2Airflow rate is 1~100mL/min, and argon stream speed is 10~1000mL/
Min, vapour deposition temperature is 700~1000 DEG C, and vapor deposition times are 0.5~5h.
3. the preparation method of sandwich structure C-base composte material according to claim 1, it is characterised in that the step
(2) in, soluble nickel salt is the one or more in nickel chloride, nickel nitrate and nickel acetate, and the concentration of soluble nickel salting liquid is
0.01~1mol/L.
4. the preparation method of sandwich structure C-base composte material according to claim 1, it is characterised in that the step
(1) in, the temperature of carbonization treatment is 500~1200 DEG C；The time of carbonization treatment is 0.5~5h.
5. the preparation method of sandwich structure C-base composte material according to claim 1, it is characterised in that the step
(1) in, zincum salts pore creating material is the one or more in zinc acetate, zinc chloride and zinc nitrate.
6. the preparation method of sandwich structure C-base composte material according to claim 5, it is characterised in that the step
(1) in, the mass ratio of chitosan and zincum salts pore creating material is 1：(0.01~1).
7. the preparation method of sandwich structure C-base composte material according to claim 1, it is characterised in that the step
(2) in, the time of immersion is 1~20h.
8. a kind of sandwich structure C-base composte material, it is characterised in that the C-base composte material is by claim 1~7
Any one of them preparation method is prepared；The C-base composte material forms three by graphitization carbon-coating cladding amorphous carbon layer
Mingzhi's structure, its outer layer are graphitized carbon material, and internal layer is amorphous carbon material.
9. sandwich structure C-base composte material according to claim 8, it is characterised in that the thickness of the graphitization carbon-coating
Spend for 1~100nm, the thickness of the amorphous carbon layer is 10~200nm.
10. a kind of application of sandwich structure C-base composte material as claimed in claim 8 or 9, it is characterised in that made
It is applied to for negative material in sodium-ion battery.
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| CN109167071A (en) * | 2018-08-31 | 2019-01-08 | 深圳大学 | A kind of cathode for whole vanadium oxide reduction flow battery and preparation method thereof |
| CN111408392A (en) * | 2019-01-08 | 2020-07-14 | 南京理工大学 | Cobalt-nitrogen co-doped porous carbon material catalyst and preparation method and application thereof |
| CN113013391A (en) * | 2021-02-23 | 2021-06-22 | 北京工业大学 | Method for preparing nitrogen-doped multidimensional and hierarchical porous carbon material adaptive to sulfur anode carrier of aluminum-sulfur battery |
| CN113113600A (en) * | 2021-04-06 | 2021-07-13 | 常德速碳新能源科技有限公司 | Negative electrode material for lithium ion secondary battery and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109167071A (en) * | 2018-08-31 | 2019-01-08 | 深圳大学 | A kind of cathode for whole vanadium oxide reduction flow battery and preparation method thereof |
| CN111408392A (en) * | 2019-01-08 | 2020-07-14 | 南京理工大学 | Cobalt-nitrogen co-doped porous carbon material catalyst and preparation method and application thereof |
| CN113013391A (en) * | 2021-02-23 | 2021-06-22 | 北京工业大学 | Method for preparing nitrogen-doped multidimensional and hierarchical porous carbon material adaptive to sulfur anode carrier of aluminum-sulfur battery |
| CN113113600A (en) * | 2021-04-06 | 2021-07-13 | 常德速碳新能源科技有限公司 | Negative electrode material for lithium ion secondary battery and preparation method thereof |
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| Publication number | Publication date |
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| CN107994222B (en) | 2020-06-09 |
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